Scientia et Technica Año XXVII, Vol. 27, No. 04, octubre-diciembre de 2022. Universidad Tecnológica de Pereira. ISSN 0122-1701 y ISSN-e: 2344-7214
223
Abstract In this study, a low-cost simple manufacturing process
for a composite material of thermoplastic matrix
PolyEtherEtherKetone (PEEK) and carbon fiber (CF) was
developed. The composite material CF/PEEK was mechanically
evaluated by three-point bending and tension tests, obtaining the
elastic modulus and the maximum tensile stress respectively. Also,
threads were made in the composite material and the strength of
threads machined on the composite material was evaluated with
tension tests. A comparison of the composite material CF/PEEK
and the composite material of carbon fiber and epoxy resin
(CF/EP) was performed, the elastic modules, peak tensile stresses
and the strength of threads were compared. It was found that it
was possible to produce the CF/PEEK composite at low cost by hot
molding. The elastic modulus and tensile strength of the CF/PEEK
were lower than those obtained in the CF/EP. However, the
performance of the thread in tension was better for CF/PEEK
compared to CF/EP.
Index Terms Carbon Fiber, Epoxy Resin Manufacture,
PEEK, Mechanical Characterization, Thread.
ResumenEn este estudio se desarrolló un proceso de
manufactura sencillo, de bajo costo para producir un material
compuesto de matriz termoplástica PolyEtherEtherKetone
(PEEK) y fibra de carbón (CF) mediante moldeo en caliente. Se
caracterizó mecánicamente el material compuesto CF/PEEK con
ensayos de flexión en tres puntos y tensión, se obtuvieron el modulo
elástico y la resistencia máxima a tensión, respectivamente.
También roscas fueron maquinadas en el material compuestos y
se evaluó la resistencia de estas roscas mediante pruebas de
tensión. Se reali una comparación del material compuesto
CF/PEEK con el material compuesto de fibra de carbón y resina
epoxi (CF/EP), los módulos elásticos, la resistencia máxima a la
tensión y la resistencia de las roscas fueron comparadas. Se
encontró que fue posible producir a bajo costo mediante moldeo al
caliente este compuesto de CF/PEEK. El módulo elástico y la
resistencia a la tensión fueron menores que las obtenidas en el
CF/EP. Sin embargo, el desempeño del CF/PEEK a tensión en
las roscas fue mejor comparado con el compuesto de CF/EP.
This manuscript was sent on June 30, 2021 and accepted on November 21,
2022.
J. E. Caicedo-Zuñiga, M.Sc. is with the Mechanical Engineering School,
Universidad del Valle, Cali, Colombia). (e-mail:
joyner.caicedo@correounivalle.edu.co).
Palabras claves Caracterización mecánica, Fibra de carbón,
Manufactura, PEEK, Resina epoxi, Roscado.
I. INTRODUCTION
IBER reinforced materials are currently used in several
applications as for example, in the aerospace, automotive,
and biomedical engineering due to their good mechanical
properties combined with a relatively low weight [1]. Fiber
reinforced polymers (FPR) as composite materials are a good
strengthening technique for a variety of structural applications
and have been the focus of research in recent years. FPR were
performed as high performance materials because of their
advantages such as light weight, fatigue resistance, high tensile
strength, corrosion and thermal insulation [2]. These materials
are composed of fibers impregnated with a thermoset or
thermoplastic polymer matrix. When a thermoplastic polymer
is heated, their chemical bonds are broken causing a change of
state from solid to high viscosity liquid. In this state this
material can be deformed inside a mold where it is subsequently
cooled to solidify and obtain a mold-shaped piece [3].
PolyEtherEtherKetone (PEEK) is a thermoplastic polymer with
good mechanical properties frequently used as a matrix in
composites materials [4]. One of the main characteristics of the
PEEK is its high melting temperature until 400°C, which makes
it suitable for applications at relatively high temperature. In
many countries, the production of parts made of carbon fiber
reinforced with PEEK (CF/PEEK) is no completely developed
due to low availability of equipment required in the process of
autoclave, Automated Tape Laying (ATP) and Laser
Automated Tape Laying (LATP) [3]. In developing countries,
the situation is even more complex due to the slow process of
importing raw materials. However, manufacturing techniques
have been designed for these thermoplastic composites with
acceptable results. Some techniques such as: hot molding
[5][6][7], injection molding [6][8] and fused deposition
G. F. Casanova-Garcia, Ph.D. is with the Mechanical Engineering School,
Universidad del Valle, Cali, Colombia. (e-mail:
Gonzalo.casonova@correounivalle.edu.co).
Manufacture and mechanical characterization of
composite material of carbon fiber with matrix
of PEEK
Manufactura y caracterización mecánica de material compuesto de fibra de carbon
con matriz termoplástica PEEK
J. E. Caicedo-Zuñiga ; G. F. Casanova-García
DOI: https://doi.org/10.22517/23447214.24826
Scientific and technological research article
F
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modeling [9] [10] [11] are manufacturing techniques that have
been implemented to obtain composite materials at a low cost.
With the development of these techniques, in developing
countries composite materials are being manufactured and used
in applications such as: in bioengineering with the development
of prostheses for amputees [12] and in the development of
aircraft parts in Indonesia [13]. While in other countries, such
as: Brazil, Nigeria, India and Pakistan use natural fibers to make
biocomposites materials [14] [15] [16] [17].
Some authors who used hot molding to manufacture composite
materials with a thermoplastic matrix were Batistas et al. [18],
In their research, they manufacture sheets of carbon fiber (CF)
reinforced with polyphenylene sulfide (PPS), they vary the
cooling speed and compare the mechanical properties of these
speeds, Kaya et al. [19], Made composite panels in PLA with
basalt fibers (BF), they varied the fiber content to find high
mechanical properties and Mazur et al. [C], Found in their
research that hot molding is a good alternative to making the
composite material with a thermoplastic matrix of
polyetherketoneketone (PEKK) and carbon fiber with
appropriate impregnation.
The biggest challenge in the manufacturing process of
thermoplastic matrix composites is to achieve the appropriate
stamping temperature, this is the most important factor that
affects the quality of processing and the performance of these
composites, for example, by increasing temperature can cause
porosity, but too high a temperature will cause the matrix to
decompose and increase porosity [7]. On the other hand, the
cooling speed achieved with hot molding is also another
challenge when processing these materials, since it affects the
mechanical properties of the final product [6][7].
This paper presents a methodology to produce fiber-reinforced
material and thermoplastic matrix at high temperatures, through
a low-cost process, where a composite material with acceptable
mechanical properties was obtained. The objective of this study
was to produce CF/PEEK without conventional and expensive
equipment and compare it with carbon fiber composite material
and epoxy resin (CF/EP), especially the strength of machined
threads for the use of bolted joints.
II. MATERIALS AND METHODS.
A. Materials
Carbon fibers are frequently used as reinforcement material due
to their high mechanical properties. Fibers with tension
modules ranging from 207 GPa to 1035 GPa are currently
available [21]. In this study, for the manufacture of the
composite material we used fabric made of carbon fiber 3K
reference HexForce 282 (Hexcel Corporation, Stamford, CT,
USA), where the fibers follow an orientation pattern in the
and 90° directions and a plain weave style. According to
manufacturer [22], this fabric has a thickness of 0.26 mm, a
tensile strength of 3650 MPa and elastic modulus of 234 GPa.
PEEK was chosen as matrix since it offers the possibility of
being used at high service temperatures (until 250°C). It has an
elastic modulus of about 4 GPa, a yield stress of 100 MPa, and
has a higher fracture toughness in comparison with the epoxy
resin [23]. Filaments of PEEK with 1.75 mm diameter (Apium
Additive TechnologyGmbh, Germany) were used as matrix.
While for the composite with thermosetting matrix, epoxy resin
744 was used.
B. Fabrication process
Hot compression molding was the selected manufacturing
process since it is one of the lowest cost process due to the use
of required equipment. This process begins with cutting a
rectangular section of fabric. Then, PEEK filaments were added
onto the fabric, followed by another layer of fabric laid over the
PEEK filaments and so on until eight layers of fabric and eight
layers of PEEK filaments were completed.
These layers of PEEK fabric and filaments were stacked and
compressed inside a mold made of AISI 1020 steel plates with
dimensions 150 mm x 150 mm x 4 mm and an electrical
resistance that works at 110 V at the base. The composite
material manufacturing process took 90 min. The parameters
used during this thermal cycle were: temperature 380 °C,
pressure 0.47 MPa and cooling rate 2.2 °C/min. Pressure was
applied gradually, while heating the mold, using a Hubbard-
field mechanical vise (Hubbard-field, Gainesville, FL, USA)
with a 10000-pound capacity. The CF/PEEK pieces obtained
were between 4 and 6 mm thick and presented a good surface
finish. These pieces were cut with a band saw to obtain 15 mm
x 150 mm specimens for bending tests and 25 mm x 150 mm
for tensile tests (Fig. 1a). The FC/EP was manufactured by
Hand Lay-Up [24].
C. Fiber weight fraction
The fiber weight fraction in the composite material resulting
from compaction and heating process was calculated by using
(1) [25].
 
 (1)
Where
and
are the weights of the fabric used and matrix
respectively. For CF/PEEK the following procedure was
performed to determine the weights mentioned above. First, the
carbon fiber fabric and PEEK filaments needed for the
composite material were weighed. Then, the compaction and
heating process take place, and then the residual PEEK from the
hot compression process was removed which was filtered from
Scientia et Technica Año XXVII, Vol. 27, No. 04, octubre-diciembre de 2022. Universidad Tecnológica de Pereira.
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the mold. Finally, the final product resulting from the CF/PEEK
composite manufacturing process was weighted. While for the
CF/EP composite, the weight fraction of the fiber was
calculated with the initial weight of the fabric introduced into
the mold, and compared with the final weight of the piece
impregnated with the cured resin.
Total fiber volume fraction is calculated by using (2) following
as [25] [26]:

(2)
Here,
and
are the densities of the fabric used and matrix
respectively.
D. Mechanical tests
Three-point bending tests and tensile tests were performed on
samples of the composite materials to determine their elastic
modulus and ultimate strength. Also the strength of a thread
machined on the composite material was evaluated by tensile
tests as explained below. Three specimens were evaluated for
each kind of test.
Based on the ASTM D7264 standard [27], this standard
recommended a strain range of 0.002 with a start point 0.001
and end point 0.003, therefore, only the valid elastic region of
stress-strain curve was registered. The specimens were
subjected to three-point bending tests as shown in Fig. 1b. The
two endpoints were simply supported while the load was
applied at the midpoint. The tests were performed on a testing
machine reference Lloyd LF plus instruments (AMETEK TCI,
FL, USA). A displacement of two millimeters was applied to
characterize the linear elastic zone of the material avoiding any
damage to the specimens. Displacement was measured with a
(1) LVDT reference LD620-7.5 (Omega Engineering Inc,
Norwalk, CT). The force was measured with a tension-
compression load cell type S NTEP (2). Data were registered
with a DC 204R data acquisition system (TML, Tokyo Sokki
Kenkyujo Co., Ltd., JP) with a sampling rate of 100 Hz.
According to ASTM D7264 the stress (σ) in the middle of the
specimen is calculated with the force by using (3):
 
(3)
Where P is the applied force, L is the distance between supports,
b is the width of the specimen and h is the thickness. In addition,
the strain (ε) in the center was calculated by using (4):

(4)
Where δ is the deflection at the midpoint.
The elastic modulus was determined as the slope of the linear
zone of the stress-strain curve.
Tensile tests were performed under the ASTM D3039 standard
[28]. The tests were carried out in a universal Tinius Olsen
H50KS test machine (Fig. 1c), to characterize the material
ultimate tensile stress.
According to ASTM D3039 standard [28], the ultimate tensile
stress (

) recorded at the failure of the specimen is calculated
by using (5):


(5)
Where

is the maximum force reached just before the
fracture and A is the cross-sectional area of the specimen.
The strength of a machined thread on the composite material
was also evaluated. To generate the thread, an  
in hole
was drilled in the composite material and subsequently an
in tap with ordinary thread was introduced. An
in bolt was
inserted into this thread where a tensile test was performed on
the Tinius Olsen H50KS universal testing machine based on
ASTM F549-17 [29]. For the tests, an assembly was
constructed (Fig. 1d) in which a fixed base (1) maintains the
threaded area of the composite material (2) confined while the
cover (3) top supports the test piece with bolts. With the screw
(4) the force is applied.
Fig.1. a) Specimens for mechanical tests I) Bending test, II) Tensile test. b)
Three-point bending tests. c) Tensile test. d) Tensile testing scheme in
composite thread
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III. EXPERIMENTAL DESIGN
A completely randomized experimental design was used for
one factor: the composite material, with two levels: CF/PEEK
and CF/EP, using three replications per treatment. Six
specimens for each composite material were mechanically
evaluated: three using bending test and three using tensile test.
Variable responses were the elastic modulus and the ultimate
tensile stress.
Statistical analyses of variance were conducted for the elastic
modulus and ultimate tensile stress with confidence level of
95%.
IV. RESULTS
To validate the analyses of variance, Ryan-Joyner (similar to
Shapiro-Wilks) test was performed with p-values greater than
0.1 for the two analyses performed. In addition, we performed
Levene test with p-values of 0.264 for the analyses of the elastic
modulus and p-values of 0.386 for the analyses of the tensile
ultimate strength results. The independence was guaranteed by
randomize the sequence of the tests.
The fiber weight fraction achieved for the CF/PEEK composite
was 44.3%, while for the CF/EP was 65.4%. Both CF/PEEK
and CF/EP specimens showed an elastic linear behavior (Fig.
2) under the test conditions (only in the elastic region). For the
CF/PEEK an average elastic modulus of 8.35 GPa was found
with a standard deviation of 0.82, this value is within the elastic
modulus of the matrix and the reinforcement, while the CF/EP
material presented an average elastic modulus of 20.7 GPa with
a standard deviation of 8.54.
Fig. 2. Typical stress vs. strain curve obtained in FC/PEEK and CF/EP
specimens tests
An analysis of variance (Anova) (Table I) showed that the
difference between those average values was statistically no
significant (p-value >0.05), probably due to the low number of
specimens used for the tests, three for treatment.
TABLE I.
ANOVA ELASTIC MODULUS
Source
Ms
p
Composite
Material
232.88
6.32
0.066
Error
36.85
Total
The average ultimate tensile strength of the CF/PEEK
composite materials was 256.4 MPa with a standard deviation
of 117.8 MPa, this high standard deviation could be due to the
manufacture of the composite material, the bond between
PEEK layers and carbon fiber cloth, and for the CF/EP the
average was 365.4 MPa with a standard deviation of 21.2 MPa.
An analysis of variance (Table II) showed that the difference
between those average values was statistically no significant (p-
value = 0.308). The tensile tests were conducted only to obtain
the tensile strength of the material; therefore, the strain was not
registered during these tests and the corresponding stress-strain
diagrams were not obtained.
TABLE II.
ANOVA ULTIMATE TENSILE STRENGTH
Source
Ms
p
Composite
Material
14153
1.50
0.308
Error
9429
Total
For comparison purposes, Table III presents the results of
elastic modulus and ultimate strength obtained for the
CF/PEEK material together with other recent investigations.
The elastic modulus and ultimate strength obtained was smaller
than most of the values reported by other studies. However, the
cost of the manufacturing process proposed in this study is low
and this composite material could be carried out successfully.
Low values of mechanical strength and ultimate tensile can be
explained by the fiber volume low fraction and the adhesion
between the layers of fabric and matrix obtained with the
process presented in this paper in comparison with those
reported in the literature. Chunrui et al. [30] obtained greater
elastic modulus and tensile strength, probably because they
manufactured the composite material CF/PEEK starting from
layers of fabric made from yarns of PEEK and carbon fibers,
which have good adhesion of peek in the carbon fiber, improved
by the applied pressures of 0.5 MPa. Elwathing et al. [31], also
obtained a material with greater elastic modulus than the
obtained in the present study, probably due to chemical
activation process in the carbon fiber with acid, combined with
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a manufacturing process using pressures and cooling rate of 2.5
MPa and 20 °C/min respectively. Shang-Lin [32] and Sharma
et al. [33], manufactured composite material of CF/PEEK using
carbon fiber and powder of PEEK. While Shang-Lin [32]
obtained a material with relatively low elastic modulus, Sharma
et al. [33] obtained a material with better mechanical properties
probably explained by the thermal cycle and the compression
using a pressure of 0.7 MPa.
TABLE III.
COMPARISON OF RESULTS CF/ PEEK COMPOSITE
Researcher
Fiber
Volume
Fraction
Fiber
Weight
Fraction
E
(GPa)

(MPa)
Year
In this paper
36.8
44.33
8.35
256.4
2019
Lu et al. [30]
40.3
-
48.9
480.7
2018
Elwathing et
al. [31]
40
-
23.5
-
2018
Shang-Lin et
al. [32]
61
-
4.5
140.2
2000
Sharma et al.
[33]
-
68
51
576
2011
The maximum force reached in the tensile tests on the threads
made in the CF/PEEK composite material reaches an average
of 5.6 KN with a standard deviation of 0.75 and for the CF/EP
the average was 2.6 KN with a standard deviation of 0.79. The
CF/PEEK composite was significantly better than the CF/EP
for this application (p-value = 0.011) as shown in table IV.
TABLE IV.
ANOVA TENSILE ON THE THREADS
Source


Ms
p
Composite
Material
11358544
1
11358544
20.42
0.011
Error
2225118
4
556279
Total
13583662
5
The CF/PEEK composite material showed a lower modulus of
elasticity and a lower ultimate tensile strength, compared with
the CF/EP composite as shown in table V. This is probably due
to the fact that in the CF/PEEK composite it was not possible to
obtain a fiber weight fraction as high as was achieved in the
CF/EP composite. The performance of the CF/PEEK material
was greater in the maximum force reached in the threads, which
may be due to a greater shear resistance of the PEEK with
respect to the EP. This makes the CF/PEEK material a
promising material in the manufacture of threaded joints.
TABLE V.
COMPARISON OF RESULTS CF/ PEEK AND CF/EP COMPOSITES
Composite
Fiber
Weight
Fraction
E
(GPa)

(MPa)



on the
threads
CF/PEEK
44.33
8.35(0.82)
256.4(117.8)
5.6(0.7)
CF/PEEK
65.4
20.7(8.5)
365.4(21.2)
2.6(0.8)
Data in parentheses are standard deviations
V. CONCLUSIONS
It was possible the manufacture of composite material of
CF/PEEK without the conventional machines and at a low cost,
additionally, this composite material presented mechanical
properties similar to those reported by other authors. A linear
behavior was evident between the stress and the strain in all the
bending tests, for the evaluated range up to strain of 0.0012
(only in the elastic region) on the two composite materials.
Regarding the effective elastic modulus and ultimate tensile
strength, the CF/PEEK composite material was no better than
the CF/EP composite material, a 60% lower effective elastic
modulus and an ultimate tension 1.37 times lower for the PEEK
compound compared to the EP compound. However, there are
still opportunities to improve properties for the CF/PEEK
composite material since by optimizing the manufacturing
process, for example, by improving the adhesion of the PEEK
in the carbon fiber, layering prepreg first, and increasing the
weight fraction of carbon fiber.
The machining process of holes and threads in the composite
material CF/PEEK was carried out with good results. The
thread strength of the CF/PEEK reached values 2.15-fold higher
than in the CF/EP composite. Therefore, the PEEK allows to
use bolted joints more resistant in the composite material.
Therefore, we can conclude that using this composite material
in parts and geometries that require bolted joints guarantees
better resistance than in composite material CF/EP.
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Joyner Esteban Caicedo Zuñiga.
Engineer Caicedo received the title of
Mechanical Engineer in 2016 from the
Universidad del Valle. In 2019, he graduated
in the Master’s Degree in Mechanical
Engineering at the same institution.
Currently, he works as a researcher for the
Energy Sustainability Alliance for Colombia
(SÉNECA).
ORCID: https://orcid.org/0000-0001-5245-3464
Gonzalo Fernando Casanova Garcia.
Professor Casanova received the title of
Mechanical Engineer in 2003 from
Universidad del Valle. In 2006, he
graduated in the Master’s Degree in
Mechanical Engineering from Universidad
del Valle. Later, he obtained a Ph. D. in
Mechanical Engineering at University of
Florida, United States, in 2013.His dissertation dealt with the
influence of needle insertion speed on tissue damage and
backflow during convection enhanced delivery of drugs in the
brain. Currently, his main research areas are: fatigue analyses
of mechanical systems, soft tissue mechanics, and mechanics of
fiber reinforced materials, including the development of
devices for orthopedic applications. His teaching areas are
focused on dynamics, mechanical design, advanced calculus,
and continuum mechanics.
ORCID: https://orcid.org/0000-0002-3146-2027